CN109553743A - A kind of Inorganic Fillers Filled high temperature resistant foamed material and preparation method thereof - Google Patents
A kind of Inorganic Fillers Filled high temperature resistant foamed material and preparation method thereof Download PDFInfo
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- CN109553743A CN109553743A CN201710872668.9A CN201710872668A CN109553743A CN 109553743 A CN109553743 A CN 109553743A CN 201710872668 A CN201710872668 A CN 201710872668A CN 109553743 A CN109553743 A CN 109553743A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1035—Preparatory processes from tetracarboxylic acids or derivatives and diisocyanates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
- C08G18/6415—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63 having nitrogen
- C08G18/6438—Polyimides or polyesterimides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides a kind of Inorganic Fillers Filled high temperature resistant foamed material and preparation method thereof, is prepared by dianhydride, polyalcohol, isocyanates, is related to polymeric foamed material field.Preparation method of the invention includes: that inorganic particulate (silicon carbide, expansible graphite, vermiculite, graphene oxide etc.) mixes with performed polymer, polymerize, Post isothermal treatment.The present invention uses deionized water for foaming agent, and inorganic particulate has high thermal stability and flame retardant property as high temperature resistant, fire-retardant phase, gained foam, and dimensional stability also improves.Inorganic Fillers Filled high temperature resistant foamed material of the present invention, it is environmentally friendly without using fluorine-containing foaming agent and toxic fire retardant, foaming process.Compared with other high temperature resistant foams: deionized water is environmental-friendly as foaming agent, and inorganic particulate is as fire retardant without pernicious gas, and heat-resisting quantity is good, and forming method is simple, has wide application and development prospect.
Description
One, technical field:
The present invention relates to heat-resisting, fire retardation polymer foam material fields, and in particular to is improved using inorganic particulate as filler
Polyurethane acid imide foam material is heat-resisting and flame retardant property and preparation method thereof.
Two, background technique:
Imide-urethane be it is a kind of chemically polyurethane and polyimides are connected on same main chain, make point
Possess polyurethane and polyimide portion simultaneously on sub- main chain, wherein soft segment is polyurethane portion, and hard section is polyimide portion.
Polyurethane is that a kind of relative mass is light, and thermal coefficient is low, and intensity is high, and sound absorption effect is good, but heat resistance is low, incendive one
Kind polymer.And polyimides is the half trapezoidal aromatic heterocyclic polymer with imide ring, from the fire-retardant angle of structure, point
Minor structure itself have it is excellent from flame-retardant nature but most of polyimides molten or fluidity of molten is not poor, it is difficult to be processed into
Type and expensive, is only used for some special occasions.So imide-urethane combines the two advantage, not only have high-strength
It spends, from excellent performances such as fire-retardant, high-low temperature resistant, resistances to oxidation, also there are the characteristics such as light, thermal coefficient is low, sound absorption to be widely applied
In the high-tech areas such as Aeronautics and Astronautics and ship, furthermore also possess broad application prospect in fields such as heat preservation, sound absorptions.
Inorganic particulate is a kind of natural material, such as silicon carbide, expansible graphite mostly.Silicon carbide (SiC) is Si-C key
The stronger covalent key compound of power has diamond lattic structure, 75 kinds of crystal forms.Silicon carbide has high thermal conductivity, and high-melting-point, low-heat is swollen
The advantages that swollen coefficient, intensity is a kind of ceramic refractory, structural material and heat sink material.Have yield big in the market, valence
The advantages such as lattice are low.Expansible graphite (EG) be it is a kind of by natural flake graphite by chemical oxidization method or electrochemical oxidation process
A kind of compound between graphite layers obtained after reason.The advantages of EG be it is nontoxic, anti-corrosive properties, cigarette is few, weatherability, is widely used in each
Halogen-free environment-friendlyflame flame retardant is served as in kind material.Application market mainly has insulating board for building, fireproof antistatic coating fire proof seal
Item etc..Such inorganic filler is added to the mechanics and thermal property that material can be improved in foamed material.However, about poly- ammonia
Ester acid imide hybrid composite material and preparation method thereof has no relevant report.
Three, summary of the invention:
The present invention solves the technical problem of a kind of polyurethane acid imide foam material is disclosed, by dianhydride, polarity
Solvent, polyalcohol, isocyanates are prepared, and are related to polymeric foamed material field.Imide-urethane foam material of the present invention
Material is using deionized water as foaming agent, and the shortcomings that overcome existing fluorine-containing foaming agent to destroy atmospheric ozone layer, it is Chinese right to meet
In the demand of environmental protection and sustainable development, environmental-friendly, nontoxic non-ignitable, foam process is simple, and expansion ratio is controllable.It is basic herein
On, the flame-resistant high-temperature-resistant performance of imide-urethane is mutually improved as heat-resistant fireproof using inorganic particulate.
The specific technical solution of the present invention is as follows:
A kind of Inorganic Fillers Filled polyurethane acid imide foam material is molten by dianhydride, polyalcohol, isocyanates, polarity
Agent, foaming agent, foam stabilizer, catalyst preparation form.
The primary blowing agent of the high temperature resistant foamed material of the Inorganic Fillers Filled is deionized water.
The main dianhydride of the high temperature resistant foamed material of the Inorganic Fillers Filled be pyromellitic acid anhydride, 3,3 ', 4,
One of 4 '-benzophenone tetracarboxylic dianhydrides are a variety of.
The high temperature resistant foamed material of the Inorganic Fillers Filled, main polyalcohol be polyether polyol, polyester polyol,
One of biopolyol (castor oil, rapeseed oil etc.) etc. is a variety of.
The high temperature resistant foamed material of the Inorganic Fillers Filled, dominant catalyst are triethanolamine, triethylene diamine, two
Laurel dibutyl tin, stannous octoate it is one or more.
The high temperature resistant foamed material of the Inorganic Fillers Filled, dominant polarity solvent are dimethylformamide, dimethyl
One of acetamide, tetrahydrofuran/methanol mixed solution, N-Methyl pyrrolidone are a variety of.
The high temperature resistant foamed material of the Inorganic Fillers Filled, principal surfactant are the copolymerization of efficient silicone ethylene glycol
Object, silicone stabilizer, silicone polyether copolymer, one of organosilicon or a variety of.
The inorganic particulate be for one of silicon carbide, expansible graphite, vermiculite, graphene oxide or a variety of, it is excellent
Be selected as: one of silicon carbide, expansible graphite are a variety of.
The foam process of the high temperature resistant foamed material of the Inorganic Fillers Filled is as follows: by dianhydride, polar solvent, isocyanide
Polyimide prepolymer is made in acid esters, catalyst, is later uniformly mixed polyalcohol, foaming agent, surfactant, inorganic particulate
And with polyimide prepolymer high-speed stirred free foaming, after inorganic particle filled high temperature resistant foam is after heat treatment made.
Four, Detailed description of the invention:
Fig. 1 is that SiC prepared by embodiment 1 and embodiment 2 fills high temperature resistant foamed material hot weightless picture
Fig. 2 is that EG prepared by embodiment 5 and embodiment 8 fills high temperature resistant foamed material hot weightless picture
Fig. 3 is that SiC prepared by comparative example and embodiment 1,2,5,8 and EG fill high temperature resistant foamed material limit oxygen index table
Five, specific embodiment:
The present invention is specifically described below by embodiment, it is necessary to be pointed out that the present embodiment is served only for pair again
The present invention further illustrates, should not be understood as limiting the scope of the invention.
Embodiment 1
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, 5 parts of silicon carbide (are accounted for about into entirety
2.4%) it is put into reaction vessel high speed and stirs to get solution B, mixing speed 2000r/min；Mixing time is 2 minutes.It will
Solution A and solution B mixing and the uniform simultaneously free foaming of high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30 seconds.
Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains inorganic grain
Son filling high temperature resistant composite foam.
Embodiment 2
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, silicon carbide 10 (are accounted for about into entirety
4.8%) part is put into reaction vessel high speed and stirs to get solution B, and mixing speed is that 2000r/min mixing time is 2 minutes.It will
Solution A and solution B mixing and the uniform simultaneously free foaming of high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30 seconds.
Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains inorganic grain
Son filling high temperature resistant composite foam.
Embodiment 3
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, 15 parts of silicon carbide (are accounted for about into entirety
7.2%) it is put into reaction vessel high speed and stirs to get solution B, mixing speed 2000r/min；Mixing time is 2 minutes.It will
Solution A and solution B mixing and the uniform simultaneously free foaming of high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30 seconds.
Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains inorganic grain
Son filling high temperature resistant composite foam.
Embodiment 4
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, 20 parts of silicon carbide (are accounted for about into entirety
9.6%) it is put into reaction vessel high speed and stirs to get solution B, mixing speed 2000r/min；Mixing time is 2 minutes.It will
Solution A and solution B mixing and the uniform simultaneously free foaming of high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30 seconds.
Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains inorganic grain
Son filling high temperature resistant composite foam.The thermal weight loss and limit oxygen index figure of SiC filling high temperature resistant foamed material prepared by the present invention
See attached drawing 1 and attached drawing 3.
Embodiment 5
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, 5 parts of expansible graphite (are accounted for about whole
Body 2.4%) it is put into reaction vessel high speed and stirs to get solution B, mixing speed 2000r/min；Mixing time is 2 minutes.
Solution A and solution B are mixed into the uniform simultaneously free foaming of simultaneously high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30
Second.Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains nothing
The particle-filled high temperature resistant composite foam of machine.
Embodiment 6
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, 10 parts of expansible graphite (are accounted for about whole
Body 4.8%) it is put into reaction vessel high speed and stirs to get solution B, mixing speed 2000r/min；Mixing time is 2 minutes.
Solution A and solution B are mixed into the uniform simultaneously free foaming of simultaneously high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30
Second.Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains nothing
The particle-filled high temperature resistant composite foam of machine.
Embodiment 7
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, 15 parts of expansible graphite (are accounted for about whole
Body 7.2%) it is put into reaction vessel high speed and stirs to get solution B, mixing speed is that 2000r/min mixing time is 2 minutes.
Solution A and solution B are mixed into the uniform simultaneously free foaming of simultaneously high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30
Second.Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains nothing
The particle-filled high temperature resistant composite foam of machine.
Embodiment 8
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant, 20 parts of expansible graphite (are accounted for about whole
Body 9.6%) it is put into reaction vessel high speed and stirs to get solution B, mixing speed 2000r/min；Mixing time is 2 minutes.
Solution A and solution B are mixed into the uniform simultaneously free foaming of simultaneously high-speed stirred.Mixing speed is 2000r/min.Mixing time is 30
Second.Resulting materials are put into baking oven and are heat-treated.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains nothing
The particle-filled high temperature resistant composite foam of machine.
The thermal weight loss and limit oxygen index of EG filling high temperature resistant foamed material prepared by the present invention are shown in attached drawing 2 and attached drawing 3.
Comparative example 1
First by 30 parts of pyromellitic dianhydride, 30 parts of dimethylformamide, 1 part of catalyst, 90 parts of isocyanates, mixing is equal
It is even, obtain solution A.17 parts of polyether polyol, 3 parts of water, 3 parts of organic silicon surfactant are put into the stirring of reaction vessel high speed
Obtain solution B, mixing speed 2000r/min；Mixing time is 2 minutes.Solution A and solution B are mixed and high-speed stirred is equal
Even and free foaming.Mixing speed is 2000r/min.Mixing time is 30 seconds.Resulting materials are put into baking oven and carry out hot place
Reason.Heat treatment temperature is 250 DEG C, and heat treatment time is 2 hours, obtains pure high temperature resistant foam.
The present invention prepares the thermal weight loss of pure high temperature resistant foamed material (0% inorganic filler) and limit oxygen index is shown in 1 He of attached drawing
Attached drawing 3.
Claims (13)
1. the present invention relates to a kind of Inorganic Fillers Filled high temperature resistant foamed materials and preparation method thereof.
2. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterised in that by dianhydride, polyalcohol, isocyanide
Acid esters, foam stabilizer, polar solvent, catalyst, is prepared without tassement polaire foaming agent.
3. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterised in that using water as foaming agent, with nothing
Machine particle is as high temperature resistant, fire-retardant phase.
4. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterized in that the dianhydride is equal benzene tetramethyl
Acid anhydrides, 3, one of 3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides or a variety of, preferably pyromellitic dianhydride.
5. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterized in that the polyalcohol is that polyethers is more
First alcohol, polyester polyol, one of biopolyol (castor oil, rapeseed oil etc.) etc. or a variety of.
6. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterized in that the catalyst is three ethyl alcohol
Amine, triethylene diamine, dibutyl tin laurate, stannous octoate it is one or more.
7. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterized in that the polar solvent is diformazan
One of base formamide, dimethyl acetamide, tetrahydrofuran/methanol mixed solution, N-Methyl pyrrolidone are a variety of.
8. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterized in that the surfactant is height
Imitate silicone glycol copolymer, silicone stabilizer, silicone polyether copolymer, organosilicon it is one or more.
9. according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1, it is characterized in that the inorganic particulate be for
One of silicon carbide, expansible graphite, vermiculite, graphene oxide are a variety of.
10. being mainly characterized by the foamed material according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1
It is prepared by following two-step method: performed polymer is made in dianhydride, polar solvent, isocyanates, catalyst, later by polyalcohol, hair
Infusion, surfactant, inorganic particulate be uniformly mixed and with performed polymer high-speed stirred free foaming, after after heat treatment be made nothing
The particle-filled high temperature resistant foam of machine.
11. being mainly characterized by the inorganic particulate according to Inorganic Fillers Filled high temperature resistant foamed material described in right 1
Number can be 1-50 parts.
12. according to preparation method described in right 10, it is characterised in that heat treatment temperature is 50-255 DEG C, and heat treatment time is
1-3 hours.
13. according to preparation method described in right 10, it is characterised in that mixing speed 1000-2000r/min, mixing time
It is 5-50 seconds.
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Cited By (3)
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| CN112920377A (en) * | 2021-01-29 | 2021-06-08 | 青岛海力威新材料科技股份有限公司 | Polyurethane soft foam material for railway solidified track bed and preparation method thereof |
| CN114058172A (en) * | 2020-08-06 | 2022-02-18 | 武汉苏泊尔炊具有限公司 | Heat insulating material, method for producing heat insulating material, and heat insulating container |
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| 王娅茹: "《HCFC-141b对聚氨酯酰亚胺泡沫材料结构与性能的影响》", 《中国塑料》 * |
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| CN111138843A (en) * | 2019-12-31 | 2020-05-12 | 苏州桐力光电股份有限公司 | Graphene-based polyurethane porous nano material and preparation method thereof |
| CN114058172A (en) * | 2020-08-06 | 2022-02-18 | 武汉苏泊尔炊具有限公司 | Heat insulating material, method for producing heat insulating material, and heat insulating container |
| CN112920377A (en) * | 2021-01-29 | 2021-06-08 | 青岛海力威新材料科技股份有限公司 | Polyurethane soft foam material for railway solidified track bed and preparation method thereof |
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